WO2005067730A1 - Procede de production de particules contenant du fer-ii-sulfate en microcapsules - Google Patents

Procede de production de particules contenant du fer-ii-sulfate en microcapsules Download PDF

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Publication number
WO2005067730A1
WO2005067730A1 PCT/EP2005/050212 EP2005050212W WO2005067730A1 WO 2005067730 A1 WO2005067730 A1 WO 2005067730A1 EP 2005050212 W EP2005050212 W EP 2005050212W WO 2005067730 A1 WO2005067730 A1 WO 2005067730A1
Authority
WO
WIPO (PCT)
Prior art keywords
particles
layer material
layer
stearic acid
temperature
Prior art date
Application number
PCT/EP2005/050212
Other languages
German (de)
English (en)
Inventor
Uwe Berlekamp
Uwe Günther
Peter Schmid
Jean-Antoine Meiners
Original Assignee
Dr. Paul Lohmann Gmbh Kg
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dr. Paul Lohmann Gmbh Kg filed Critical Dr. Paul Lohmann Gmbh Kg
Publication of WO2005067730A1 publication Critical patent/WO2005067730A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/14—Sulfates
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16—Inorganic salts, minerals or trace elements
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • A23P10/35—Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides

Definitions

  • the invention relates to a method for producing a microencapsulation of particles containing iron-II-sulfate, according to the preamble of patent claim 1 and particles containing iron-I sulfate according to the preamble of patent claim 9.
  • Mineral compounds are used for enrichment and as functional additives in food.
  • the use of microencapsulated mineral compounds is intended to protect ingredients in food from decomposition and to prevent organoleptic effects from iron minerals.
  • microencapsulated particles thereby reduce the risk of a change in color and taste of nutrients or foods containing these particles by interaction between components which are also contained in the nutrients or foods and the minerals added to them.
  • a taste and smell masking of the mineral substances is achieved by such a microencapsulation. Both properties are important, for example, in milk-based baby foods. This is intended to avoid the iron taste and taste of oxidized milk fats, such as those that arise when adding non-encapsulated iron salt.
  • microencapsulated particles have protection against external influences before and during their admixture in foods.
  • iron-Il-sulfate particles as additives in food can cause color changes in those, provided the iron-Il-sulfate-containing particles are in unencapsulated form or inadequate microencapsulation. This adversely affects the aesthetic perception of a person consuming food.
  • particles containing iron-II-sulfate rapidly convert to particles containing iron-III-sulfate through oxidation, for example through contact with oxygen as contained in the air, its effectiveness with regard to optimal absorption by the human body is maintained whose iron balance is severely impaired. Furthermore, such an oxidation affects not only the absorption but also the solubility, color, taste and durability of the iron compounds.
  • Previous microencapsulated iron-II-sulfate-containing particles have an insufficient capsule quality when used in products to be heated, such as baby foods. The consequence of this is that the microencapsulation of the particles containing iron-II-sulfate release the iron-II-sulfate prematurely and thereby cause undesired oxidation of the ingredients. As a result, redox particles form on the surface of liquids containing nutrients. This is particularly true for baby milk powder that is made with warm water.
  • the degree of such premature leakage of the microencapsulation can be determined from the number of so-called floaters that result from one that has taken place
  • the object of the present invention is to provide a method for producing a microencapsulation of particles containing iron-II-sulfate which enables the production of a microencapsulation which reliably envelops the particles, even at higher temperatures. Furthermore, it is an object of the invention to achieve microencapsulated iron-II-sulfate-containing particles with a permanent and more temperature-resistant microencapsulation. This object is achieved on the process side by the features of patent claim 1 and on the material side by the features of patent claim 9.
  • An essential point of the invention is that the following steps are carried out in a method for producing a microencapsulation of particles containing iron-II-sulfate:
  • Such a production process results in a three-layer microencapsulation of the particles containing iron-II-sulfate, which almost completely suppresses the formation of floaters up to a temperature of 62 ° C.
  • the first layer material (coating agent) is stearic acid
  • the second layer material is palm oil
  • the third layer material is again stearic acid.
  • the first, second and third layer material is melted, whereby a spray air or the atomizing air used for the spraying process is heated to a temperature of at least 90 ° C. during the spraying process and must not drop below the melting point of the fatty acids. This achieves a uniform, homogeneous and stable long-term coating of the particles.
  • the layer materials are produced with a spray rate from a range of 10-40 g / min., Preferably from a range of 12-22 g / min., And at a spray pressure from a range of 0.5 - 10 bar, preferably from a range from 1 -4 bar, applied by means of a fluidized bed system.
  • the components of the fluidized bed system which supply the layer materials are at least partially preheated by means of hot air, provided that the components are not heated.
  • Hose feed lines for the components supplying the layer materials are primarily designed to be heat-insulating by means of an insulating material or are equipped with an additional heating device.
  • the FeSO 4 x H 2 O is present in the iron-II-sulfate-containing particles as a gray-white powder. They ideally have 70-99%, preferably 86.0-89.0% FeSO 4 .
  • a ratio of FeSO 4 x H 2 O particles to the layer material of 1: 1 had proven to be a particularly advantageous mass ratio of the particles to the capsule material during the production process according to the invention.
  • the amount of material used for the first, second and third layers is determined according to the grain size of the particles so that each layer has a thickness of 10-100 ⁇ m, preferably 50 ⁇ m. k
  • a fluidized bed system is equipped with an inflow floor and a sieve insert underneath with a mesh size of 100 ⁇ m and with a two-component nozzle with nozzle openings of 1 mm.
  • Such fluidized bed systems enable the use of known fluidized bed or floating bed processes for the production of coated particles.
  • heated air is blown into a product container, which contains particles of FeSO x H 2 O on the bottom, in such quantities that the particles are separated from each other in the floating layer in a circular cycle at the two-fluid nozzle to carry out a broom sealing process with an evenly applied Layer material are passed.
  • the layer materials Before the layer materials are fed to the two-component nozzle, they are heated in a heating unit designed for this purpose. This causes the fatty acids to melt.
  • 300 g of stearic acid are atomized as the first layer material via spray air and sprayed onto the individually moving particles in the fluidizing air in the fluidized bed system. During this coating process, the coating material is kept at the set temperature.
  • the second layer of 400 g of palm oil and then the third layer which in turn comprises 300 g of stearic acid, is applied without interrupting the fluidized bed process.
  • the spray air used here has a temperature of at least 90 ° C, preferably 100 ° - 150 ° C, which corresponds at least to the melting temperature of the layer materials.
  • an analysis method was used in particular to determine the leakage value (leakage) of the coating of the particles and to determine the floaters which act as floating Particles appear on the surface of a liquid after a predetermined time - that is, a measure of the solubility of the coatings.
  • a total of three different iron-II-sulfate-containing particles were microencapsulated and analyzed, which differ mainly in the type of microencapsulation.
  • the microencapsulated particles according to the two examples from the prior art each have a single-layer palm oil coating with different layer thicknesses, whereas the embodiment according to the invention is triple-coated.
  • a weight of 0.4 g is weighed into an Erlenmeyer flask at 50% fat.
  • the sample to be measured is washed with 15 ml water and 10 ml 6N HC1 for 10 min. Let it boil until the sample is completely dissolved.
  • the solution is filtered through a pleated filter and rinsed with water.
  • the filtrate is provided with 2 drops of feroin solution acting as an indicator and titrated with cerium sulfate (0.1 N).
  • the factor Fe is 0.5585.
  • 1.0 g of sample weight is weighed into a bottle of Schoppen, provided with 3 drops of Tween 80 and 196 g of water and heated with constant shaking at 40 ° C in a water bath. After an hour, the bottle of Schoppen is cooled and the contents filtered through a pleated filter. The sample is slightly acidified and titrated against feroin solution with cerium sulfate (0.1 N). The factor Fe is 0.5585.
  • the determined value relates to the calculated weight Fe from the determination of the total iron. »
  • 1.0 g of sample weight are stirred in a 500 ml multi-necked flask under argon. During the determination, the flask is slowly heated using a water bath. A conductivity electrode measures the values of the conductivity and stores them. After the measurement, the values are sent to a PC and displayed in a curve as shown in the figure and thus evaluated.
  • 30 g of milk powder can be mixed with 22.2 mg of weight in advance. Then 180 ml of water are poured into a jam jar 15 minutes. long tempered at the respective temperature in a water bath. The milk powder mixture is suspended in the tempered water and left to stand at room temperature for three hours, in order to then determine the number of floaters floating on the surface.
  • the following table shows coated iron-II-sulfate-containing particles produced by the process according to the invention and two examples from the prior art, which do not have a three-day coating, with their values determined using the analysis method.
  • the microencapsulated particles according to the embodiment of the invention either have little or no floaters on the surface of the liquid.
  • the examples from the prior art have an uncountable number of floaters.
  • the figure shows results from the above-mentioned leakage test with conductivity under argon in a diagram which contains the conductivity in ⁇ s / cm over the temperature in ° C. to which the microencapsulated particles are exposed as values. The increases in conductivity as a function of temperature indicate a breakdown of the microencapsulation.
  • a curve 1 which shows the conductivity of a substance that consists exclusively of fully demineralized water at different temperatures, has no significant conductivity values.
  • curve 2 shows the conductivity profile of unencapsulated iron-II sulfate-containing particles at different temperatures as a reference measurement.
  • Curve 3 shows the conductivity values of the microencapsulated iron II sulfate according to example 2 and curve 4 shows the conductivity values of the microencapsulated iron II sulfate according to example 1 of the prior art.
  • Curve 5 shows the result values of the microencapsulated iron II sulfate according to the embodiment of the invention.
  • Curve 1 shows no significant conductivity values, as can also be expected for the zero sample.
  • curve 2 shows the reference measurement “iron-II-sulfate” for the conductivity profile of unencapsulated particles containing iron-II-sulfate at different temperatures.
  • Curves 3 and 4 reflect the capsule stability of the examples according to the prior art. From the increase in conductivity in curves 3 and 4 in the range of 50 ° - 58 ° C it can be seen that at a temperature of 58 ° C there is no longer a stable encapsulation of the particles. In contrast, curve 5 shows that a strong increase in conductivity only occurs above 62 ° C, from which it can be seen that the encapsulation of the particles remains stable until the particles are heated to 62 ° C.
  • microencapsulated particles according to the invention with a total of three layers of stearic acid and palm oil.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Molecular Biology (AREA)
  • Mycology (AREA)
  • Nutrition Science (AREA)
  • Biophysics (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

L'invention concerne un procédé de production d'une microcapsule de particules contenant du fer-Il-sulfate conformément aux étapes suivantes: - Chauffage d'un flux gazeux s'écoulant sur les particules à une température de 30°- 60 °C; chauffage des particules à une température de 30° - 60 °C; chauffage et fusion respectivement d'une première, d'une deuxième et d'une troisième matière en couche de type lipide à une température d'au moins 90 °C; revêtement des particules par pulvérisation de la première matière en couche qui est un premier lipide/acide gras ayant une chaîne moléculaire d'au moins 16 atomes de carbone; revêtement des particules enduites par pulvérisation de la deuxième matière en couche qui est un deuxième lipide/acide gras ayant une chaîne moléculaire d'au moins 14 atomes de carbone; et revêtement des particules enduites par pulvérisation de la troisième matière en couche qui correspond au premier lipide/adide gras. L'invention concerne également des particules contenant du fer-II-sulfate en microcapsules, les particules présentant une première couche d'acide stéarique, une deuxième couche d'huile de palme et une troisième couche d'acide stéarique.
PCT/EP2005/050212 2004-01-20 2005-01-19 Procede de production de particules contenant du fer-ii-sulfate en microcapsules WO2005067730A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004002732.3 2004-01-20
DE102004002732A DE102004002732B4 (de) 2004-01-20 2004-01-20 Herstellungsverfahren für mikroverkapselte Eisen-II-Sulfat enthaltende Partikel sowie Eisen-II-Sulfat enthaltende Partikel mit Mikroverkapselungen

Publications (1)

Publication Number Publication Date
WO2005067730A1 true WO2005067730A1 (fr) 2005-07-28

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PCT/EP2005/050212 WO2005067730A1 (fr) 2004-01-20 2005-01-19 Procede de production de particules contenant du fer-ii-sulfate en microcapsules

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DE (1) DE102004002732B4 (fr)
WO (1) WO2005067730A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2662346A1 (fr) 2012-05-07 2013-11-13 Mapei S.p.A. Additifs pour ciment Portland consistant d'un agent reducteur dans une matrice polymérique
WO2017042342A1 (fr) * 2015-09-09 2017-03-16 Dsm Ip Assets B.V. Procédé de production d'une composition comprenant des sels de métaux inorganiques physiologiquement actifs

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016191237A1 (fr) 2015-05-22 2016-12-01 The Procter & Gamble Company Agent tensio-actif et compositions détergentes contenant de la glycérine éthoxylée

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4102806A (en) * 1975-08-18 1978-07-25 Takeda Chemical Industries, Ltd. Method of producing microcapsules and resulting product
EP0411326A2 (fr) * 1989-06-30 1991-02-06 Bio-Dar Ltd. Additifs alimentaires comprenant des microcapsules et leur usage
US5589194A (en) * 1993-09-20 1996-12-31 Minnesota Mining And Manufacturing Company Method of encapsulation and microcapsules produced thereby

Family Cites Families (5)

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Publication number Priority date Publication date Assignee Title
US3035985A (en) * 1959-09-30 1962-05-22 Merck & Co Inc Chewable fatty coating of iron particles
NL6808619A (fr) * 1968-06-19 1969-12-23
JPS5323872A (en) * 1976-08-17 1978-03-04 Takeda Chem Ind Ltd Preparation of microcapsule
US4828955A (en) * 1986-10-27 1989-05-09 Japan Synthetic Rubber Co., Ltd. Microencapsulated particles and process for production thereof
DE69201589T2 (de) * 1991-04-24 1995-07-13 Unilever Nv Wachsumhüllte Partikel und Verfahren zur Herstellung derselben.

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4102806A (en) * 1975-08-18 1978-07-25 Takeda Chemical Industries, Ltd. Method of producing microcapsules and resulting product
EP0411326A2 (fr) * 1989-06-30 1991-02-06 Bio-Dar Ltd. Additifs alimentaires comprenant des microcapsules et leur usage
US5589194A (en) * 1993-09-20 1996-12-31 Minnesota Mining And Manufacturing Company Method of encapsulation and microcapsules produced thereby

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2662346A1 (fr) 2012-05-07 2013-11-13 Mapei S.p.A. Additifs pour ciment Portland consistant d'un agent reducteur dans une matrice polymérique
WO2017042342A1 (fr) * 2015-09-09 2017-03-16 Dsm Ip Assets B.V. Procédé de production d'une composition comprenant des sels de métaux inorganiques physiologiquement actifs
CN108024965A (zh) * 2015-09-09 2018-05-11 帝斯曼知识产权资产管理有限公司 生产包含生理活性无机金属盐的制剂的方法
JP2018528943A (ja) * 2015-09-09 2018-10-04 ディーエスエム アイピー アセッツ ビー．ブイ．Ｄｓｍ Ｉｐ Ａｓｓｅｔｓ Ｂ．Ｖ． 生理的に活性な無機金属塩を含む製剤の製造方法

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DE102004002732A1 (de) 2005-08-18
DE102004002732B4 (de) 2006-11-16

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